Reduction of metal compounds without fusion



Mach 25,1941.. c. HARDY REDUCTION OF METAL COMPOUNDS WITHOUT FUSIONv Filed DBC. 23, 1959 ATTORNEYS 'Patented Mar.` 25, 1941 PATENT OFFICE REDUCTION OF METAL COMPOUNDS wrrnoUT FUSION Charles Hardy, Pelham Manor, N. Y., assignor to Hardy Metallurgical Company, New York, N. Y.,

l a corporation of Delaware Application December 23, 1939, Serial 13 Claims.

This invention is'concerned with vproducing finely divided metal, particularly metal powders, by reduction of compounds of such metal (such, for example, as finely divided oxides) employing reducing gases but without substantial fusion.

In its preferred aspect, the invention contemplates the production of iron powder directly from finely divided iron oxides by means of hot hydrogen. -It aims to provide improved methods of production of metal powders, particularly iron, to the end that a clean product satisfactory for use in powder metallurgy shall be produced at low cost.

The manufacture of iron and steel objects by compressing and heat treating iron powders necessitates a clean starting material substantially 'free of Oxide iilms and non-metallic inclusions.v Iron powder of excellentvquality has been produced by electrolysis, but it is relatively expensive. Pyro-metallurgical processes-for the-production of iron powder and the like are considerably cheaper but entail operating diiiiculties. Thus, there is a tendency for incomplete reduction, due to the fact that not al1 portions of the oxidized starting material come into adequate contact with the reducing agent, with resultant inclusion of oxide or-other compounds in the product. Moreover, the iron particles as formed tend to stick together or to the walls of the receD- tacle. In consequenceof these and other operating ditliculties, the economies sought to be realized through the manufacture of iron powder of satisfactory quality by so-called sponge ironI processes have not been attained, at least to an 35. adequate extent.

the like, which has been prevalent heretofore.

Moreover, my invention in its preferred embodiment permits separation of completely reduced particles from incompletely reduced particles during the actual reduction step. 'I'his separation is such that particles which require more stringent treatment to bring about reduction remain in the reduction zone for a'longer period either by travelling therethrough at a slower rate or over a longer path so that their opportunity As aresuit of my investigations, I have dev for reduction is enhanced. Thus, my invention contemplates, in the formation of nely divided solid metal by reducing ne particles of a com- 'pound thereof with a hot reducing gas, the improvement which comprises causing a bed of 5 the particles to move along a deck upon which the bed is supported, while passing the hot reducing gas in contact with the particles and while imparting relative movement to the particles of the bed by shaking. In the preferred embodiment, the invention contemplates passing the hot reducing gas through the bed (preferv ably from below) and in any case transverse to the direction of movement of the bed while imparting a tabling movement to the bed, for example, by shaking or vibrating the deck. In.` short, in the preferred aspect of my invention the particles `to be reduced are subjected to'a tabling actionwhile being treated with the reducing gas, with the result that incompletely reduced (and consequently lighter) portions of the material tend to migrate to onev portion of Y the table or deck while completely reducedA (and consequently heavier) particles tend to migrate to another point. The completely reduced particles may be removed from the point to which they migrate as a nished product. 'I'he incompletely reduced particles 'are removed from the other portion of the deck and are, if desired, returned to the table for further treatment. 3o The apparatus of my invention in preferredl 'forms comprises a perforated deck that forms the top of a gas chambe 'I'he'perforations in the deckare so small thatA the solid particles passingl thereover are prevented from passing through them. The hot reducing gas, say, hydrogen, may be sucked through the bed into the underlying chamber but preferably the gas is forced upwardly through the bed from the chamber which is maintained under a slight positive u pressure. The apparatus is claimed in my copending divisional application Serial No. 315,963, flied. January 27, 1940. 'A .'It is preferable to preheat the material to be reduced (say, finely divided. magnetite) before 45 sending itto the table. Likewise the hydrogen or other reducing gas should be heated to reaction temperature. In the case of iron reduction the reaction is bestv conducted at temperaturesv ranging from 650i C. to 1000o C; and preferably at a temperature below 800 C., since above this temperaturev there is an increase in tendency for the sticking together of the particles. '3

The used reducing gases containing the gaseous products of reduction (say, water vapor) together 55 with excess reducing agent (say, hydrogen) may be treated to remove the products of reduction (for example, by condensation)` and then returned to the process. Thus, inthe casetof hydrogen, gases withdrawn from the reducing zone are cooled tobring about condensation of water vapor resulting from the reduction of iron oxide and the water vapor is condensed and removed from the circuit, the residual hydrogen being returned to the operation after preheating.

A variety of known forms of tabling devices may be employed. Thus,` a Sutton-Steele pneumatic table of heat-resisting construction with a porous metal deck may be employed, the -table being enclosed within a. furnace chamber. The general form of the Sutton-Steele pneumatic table is well-known and is described, for example, in Textbook of Ore Dressing, by Truscott, 1923, page 574. Other forms of pneumatic shaking tables, such as that illustrated on pages 938-v 939 of Handbook of Ore Dressing by Taggart, -l

(1927), may also b e employed.

The table may be provided with rimes or cor.- l

' corrugated metal sheet overlying the gas chamber,

with rows of line holes along the uppermost portions of the corrugations or riiiles. The deck may also be in the form of a plain or corrugated sheet made with controlled porosity by compressing and heat treating metal powders. a great number of very fine tortuous pores running through it and is admirably adapted to serve in the operation of my invention.V

A variety of motions are known for bringing about concentration or separation on shaking tables, and the invention may employ the action of pneumatic shaking tables, such as the Sutton- Steele table, or it may employ motions heretofore employed in wet tabling. A very satisfactory form of motion for a riiiled table is imparted by a pair of eccentric cams, one of which shakesthe table lengthwise and the other laterally, giving a resultant that is oblique to the riilles. The heavier particles of reduced metal tend 'to remain in the bottom of the rimes and travel to the end of the table therein. Incompletely reduced particles are lighter and tend to ride over the rimes passing to the side of the table. vAn impetus should be given to theparticles to cause them to move along the deck. This may be done by imparting a s lope to the deck, or by shaking the deck in its plane with a forward stroke that is faster than the backward stroke, or by a current of the reducing gas which blows the particles along the deck.

In the operation of my invention, the particles on the deck are kept in almost constant movement with respectto the deck and with respect to each other so that new surfaces are constantly being exposed to the action of the reducing gas. At the same time, the movement between the particles tends to inhibit sticking, provided that the temperature of operation is not too high.

These and other aspects of my invention will be more thoroughlyunderstood in the light of the following detailed description taken in conjunc- 75 tion with the accompanying single figure which is Such a sheet has a flow sheet of a preferred form, of my invention employing a shaking table having a perforated corrugated deck of heat-resistant metal.

Referring now to the figure, it will be observed that there is provided a shaking table I enclosed within a furnace or reduction chamber Il (fragmentarily shown). The shaking table has a corrugated deck I2, the corrugations of which extend parallel to each other and approximately lengthwise of the table. The ridge of each of the series of Vcorrugatons is perforated and has a series of small loles I3 running lengthwise of the ridge. The deck is disposed above and forms the top of a gas chamber Il. The shaking motion is imparted to the table by a plurality of eccentric cams.` Thus, cam I5 is mounted to bump periodically against the end of the table, while a `second cam I6 is mounted to bump periodically V against the side of the table. The table is movably mounted on conventional supports, not shown and springs or other conventional means (not shown) are provided for restoring the table to itsoriginal position after it has been bumped.

Feed to the tablel for example, a magnetite sand Vranging in size from 80 mesh to 16 mesh,- Tyler scale. is passed in a dry condition through a preheater I1 of conventional form such, for example, as a-rabbled hearth wherein it may be heated directly with a flame. The preheated feed particles at a temperature of say 700 C. are then fed gradually and continuously through a chute I8 that passes through the roof of the furnace I I, so that the feed is dropped on one end of the table adjacent its end baille I2A. Hot hydrogen gas is passed in'w the gas chamber I 4 underneath the table, passes` through the perforations or pores I3 in the deck to come in contact with the par ticles to'be reduced. 'The hydrogen may be introduced into the table chamber conveniently through a flexible connection ,It

A bed of particles is formed upon the deck of the table and tends to move away from the chute due to the shaking of the table brought about by the cams.l The hydrogen gas comes in contact with the particles of iron oxide and tends to reduce them rapidly. Particles which are completely reduced and hence are principally iron 'the table is substantially retarded and they remain in the reduction zone for a longer time, com- 'tend to travel longitudinally in the valleys ofthe ing intoJcontact with the` hot hydrogen gaswhich i issues from the holes in the deck.A If in the travel across the deck the particles become completely reduced they will tend to be delivered at the end of the table. Otherwise they pass off the rear edge of the table into a tailing collecting lchute 2l from which they may be wasted or returned to the oxide preheater I1. v

In the reaction between the iron oxide andthe hot hydrogen, water vapor is producedvand this water vapor, together with excessv hydrogen is removed from the furnace chamber II and passed to a condenser 422 wherein the gas isA cooled to the point where the water condenses` and is drained out of the system through a line 23. The uncondensed hydrogen from the conv denser, together with fresh hydrogen from an exterior source 24 is pumped by means of a conventional vapor pump through a conventional` hydrogn preheater V26 and is then returned toV the gas chamber of the table through ible connection I9.

As indicated hereinbefore, the table deck may be made as a porous metal sheet, either corrugated or plain, by powder metallurgical methods and various table shaking means other thanl the one illustrated may be employed. Y If desired, a current of gas may be blown along the table from a pipe (not shown) that is maintained under positive pressure. This gas current, together with the transverse gas current of gas forced upward through the bed tends to impart a swirling action to the lighter particles lying on the top of the bed which aids in `their reduction.

Although I have described my'invention in detail with reference to the reductionof iron oxide with hydrogen, it will .be apparent that the flexoxides and other compounds of other metalsmay be reduced in 'theprocess of my invention with various reducing gases such, for example,

` as carbon monoxide.

.metal by reducing particles of a compound of a metal with a hot gaseous reducing agent without substantial fusion, the improvement which comprises passing the hot reducing gas through a bed of the particles while on a deck, simultaneously imparting an/oscillatory motion to the deck to cause the particles to move therealong and to cause a separation of the particles thereon according to specic gravity, the hot reducing gas being passed through the bed of particles transversely to their direction of .travel along the deck, and removing the `resulting nely divided of metal by reducing particles of a compound solid metal from an end portion of the deck.

2. In the formation of finely divided pieces of metal by reducing particles of a compound without substantial fusion,

particles while on a deck, and simultaneously imparting an oscillatory motion to the deck to cause the particles to move therealong and to cause a separation of the particles thereon ac# cording to specic gravity, the hot reducing gas being passed through the bed of particles transversely to'their direction of travel, along the deck.

3. In the formation of. finely divided pieces of metal by reducing particles of a compound of a metal with a hot gaseous reducing agent with-4 out 'substantial fusion, .the improvement which comprises passing the hot reducing gas upwardly through a, bed of the particles at a plurality of points between particles while the bed is on a deck, and simultaneously impartingan oscillatory 'v particles by treatment in a hotreducing gas to form nely divided iron particles the improvemotion to .the deck'to cause the particles to move therealong and to cause a separation of the particles thereon according to specific gravity, the

vhot reducing gas being passed through the bed of particles transversely toA their direction of travel along the deck. i

4. In the formation of finely divided pieces of metal by reducing particles of a compound of a metal with a hot gaseous reducing agent without substantial fusion, the improvement which comprises passing the hot reducing gas in contact with abed of the particles disposed on a deck while'subjecting the particles to separation by tabling.

5. In the formation of finely divided pieces of metal by reducing particles of a compound of a vmetal with a-hot gaseous reducing agent without substantial fusion, the improvement which comprises passing the hot reducing gas upwardly through a bed of the particles disposed on a deck whiieimpartlng a shaking motion to the deck and causing the particles to move with respect to each other and to travel along the deck, heavier particles being removed from one portion of the deck and lighter particles being separated from the heavier particles and removed from another` portion of the deck.

6. In the formation of finely divided pieces of metal by reducing particles of a compound of a metal with ahot gaseous reducing agentI without substantial fusion, the improvement which comprises passing 'the hot reducing gas vupwardly through a bed of the particles disposed on a deck providedrwith a plurality of riles 'extending in the same general direction and-imparting an approximately horizontal -shaklng motion to the deck in a direction oblique to the riilles so that metal powders of relatively high specificl gravity formed by the reduction travel along the deck in thedirection ofthe riilles and lighter particles across the riilles.

7. In the formation of iinely divided pieces of metal by reducing particles of a compound of a metal with a hot gaseous reducing agent without substantial fusion, the improvement which containing unreduced -metal tend to travel.

comprises passing the hot reducing gas throughl a bed of said particles disposed on .the deck while moving the bed along the deck and while bringing about theA separation of particles of dierent specific gravity by shaking.

8. In the formation of finely divided pieces incompletely reduced particles from another por-v Y y tion of the table.

9. In the formation' of nely divided pieces of iron byA subjecting small particles of a compound thereof tothe action of a hot reducing gas, the improvement whichcmprises passing the hot gas through a bed of the particles on a deck while subjecting the deck to a tabling motion such that separation of particles of different specic gravity takes place on the deck.

l0. In the reduction of nely divided iron oxide ment which comprises the hot gas in contact with a bed of the. particles while subjecting the bed to a tabling motion to separate particles of high' metallic iron content from less completely reduced particles. V

11. In the formation of finely divided solid iron particles by subjecting small particles of iron oxide to the action of hot hydrogen without subiron, the improvement which comprises passing the hot hydrogen incontact with a bedv of the particles while subjecting: the bed to a tabling 75 stantial Afusion of the resulting particles of the motion to separate of relatively nigh metallic iron content from incompletely reduced particles, withdrawing the incompletely reduced i particles from one portion of the deck and returning themtothe deck. f i

12. In the formation'l of lnely divided solid iron particles by subjecting small particles of iron Y oxide te the action of not hydrogen without sul stantlal fusion of the resulting particles of iron,v

the improvement whichv comprises passing the hot hydrogen in contact with a bed of the particles while subjecting the bed to a tabling motion to separate particles-otrelatively high metullio iron content from incompletely reduced particles. withdrawing excess Ahot hydrogen containing water vapor resulting from the reduction assaut i .l f

about separation of powders containing a relatively large proportional metallic iron from relatively unreduced particles, the particles fed to the reduction Vzone being preheated.

CHARLES HARDY. 

